反应 #9227

反应方程式

1-(6-trimethylsilylacetylenyl-2-benzothiazolyl)-3-ethylurea

KOH

HCl

→

desired compound

收率 5.6%

1-(6-Acetylenyl-2-benzothiazolyl)-3-ethylurea

收率 5.6%

溶剂

MeOH

AcOEt

反应条件

后处理

1. 1
   萃取the aqueous phase was extracted with 10 mL AcOEt
2. 2
   干燥The combined organic portions were dried (MgSO4)
3. 3
   浓缩concentrated
4. 4
   其他purified by HPLC

实验过程

A mixture of 1-(6-trimethylsilylacetylenyl-2-benzothiazolyl)-3-ethylurea (0.0710 g, 0.22 mmol) and 1M aqueous KOH solution (1.22 mL, 1.22 mmol, 5.5 eq) in 1.5 mL MeOH was stirred at room temperature for about 2 hours. The mixture acidified with 1 M HCl, then taken up in 20 mL AcOEt, and the aqueous phase was extracted with 10 mL AcOEt. The combined organic portions were dried (MgSO4), concentrated, and purified by HPLC to give the desired compound 0.003 g (5%). LC/MS 246 (M+1); LC retention time 2.84 min.

来源